Production of iron oxide



ATTORNEYS P. FIREMAN `PRODUCTION OF IRON lOXIDE Patented Dec. 26, 1939 UNITED STATES PRODUCTION F IRON OXlDE Peter Fireman, Lambertville, N. J., assigner to Magnetic Pigment Company, New York, N. Y., a corporation of New York Application .my z3, 193s, serial 220,842

1 cnam. (c1. ca -zoo) This invention relates to the production of red iron oxide of predetermined sheds from commercial copper-as, and particularly to e. method of drying end calcining copperas in a, continus ous operation to produce en oxide of satisfactory quality 'containing not more then .05% of mengenees.

Commercial copperes is iron sulphate carrying 'l molecules of water oi. crystallization l0 (FeSOiHHsG). There is elweys present e smell amount of mengenese sulphete (MnSOilwhich' tends tc decompose when the conperes is celcined, to forni manganese dioxide in the product. For runny purposes the presence of manganese l5 is detrimentsl. So long es the mengenese remeins in the term of sulphate, it may be washed from4 the iron oxide product, whichis insoluble in water, but manganese in the insoluble forni of manganese dioxide cannot be removed from the product by washing.

` Heretoforev red iron oxide of low manganese content has been manufactured from copperss only by e. betch method, i. e., the copperes previously treated to remove e. partof the water of crystallization is pleced in a cylindrical rotsting furnace and heeted with e. ges or fuel oil arne for e. time sucient to decompose the iron sulphete. Sulphur dioxide and sulphur trioxide nre removed, and the meteriel is converted into iron oxide. Control .of the batch operation is felrly simple, end the product is discharged when the proper color hes been etteined. Batch opere.- tions are, however, relatively expensive, with resulting increased cost of the product.

It has not been commercially practicable heretofore to conduct the drying or dehydreting end the calcining operations in e continuous manner, wherein the materiel flows from the source to the delivery point without interruption. Such en operation requires the control of numerous fectors which aiect the result. For exemple, in calcining the dehydrated copperas, it is necessary to maintain uniformity in respect to the quantity of material treated end the time of such trentment. This, in turn, depends upon uniformity of feeding -of the dehydrated material, and entails e. uniform and constant rate of drying. Other factors will be discussed in more detail in the following description.

5`0 It is the object of the present invention to provide a method of drying and cnlcining corne mercial copperas which is continuous in the sense that the raw material enters the dryer and is delivered uniformly and Without interruption to 5L the Acelciner, where it is subjected to further heet and is discharged at substantially the rate'of feeding as the iron oxide product.

Another object of the invention is the `provision of e. method in-which 'the initial drying is carried out uniformly to remove 6 of the 7 t molecules of water, affording an intermediate product designated as l mole iron sulphate, which is fed continuously and uniformly to the celciner.

Another object of the invention isthe pro- E@ vision of a method in which commercial iron sulphate or copperas is converted in a continu.u ous operation into red iron oxide containing not more then .05% of insoluble manganese, the remaining manganese present being retained in E@ soluble form so that it cenbe washed from the product.'` v

A further object of the invention is the provision of e. method in which the raw materiel,

copperas, is subjected to counter-current flow of g@ i heatiduring the drying stage and thereafter to concurrent heating during the calcining stage, ,n with eiective control of the numerous factors end particularly the temperature gradients in the dryer and calciner, so es to accomplish the de- 2i@ sired result. f

Other objects and advantages of the invention will be apparent as it is better understood `bv reference to the following specification and the' accompanying drawing, which illustrates die.- 3,@ gremmatically the successive operations to which the raw material is subjected.

in carrying out the invention, l employ inclined cylindrical rotating furnaces through which the material is adapted to dow continuously, a. suit- 3g able conveyor being provided'between the fur neces tofeed the material from one to the other.A lin the first furnace or'dryer, copperas, which is supplied at e uniform ratefrorn a suitable source,

travels countercurrent to the name and hot gases o a resulting from the combustion of a suitable fuel such ns gas. The dehydrated material, which has lost 6 of its 7 molecules of water, is then fed uniformly and continuously to the second furnace or calclner, where itis subjected to heat 45 supplied by the flame and hot gasesfrom the combustion of a suitable fuel such as gas. In the calciner, the ame and gases travel concurrently with the material treated. By suitable regule,- tion of the temperatures in the dryer and caleiner, it is possible to complete the operation successfully and to produce a product of satisfactory color having not more than .05% off manganese in insoluble form. The product is then washed to remove the soluble manganese and o5 2 K other undle and con m mating mate-11318.

Copperas contains 45.29% of water of crystallization. If heated rapidly, it melts in this water and becomes unmanageable due to caking and majorr part of the water while leaving the material ilne and soft. This is accomplished by warming the copperas gently in air in which the relative humidity is closely controlled. For example, if too little air is used for drying, or if heat is applied too rapidly, or both, the copperas will melt. If too much air is used, or too little heat is applied, or both, much/of the dried copperas is blown out of the dryer, with resulting serious loss. I have discovered that to secure effective g without either of the diiiculties mentioned, it is necessary to maintain temperatures so that the air leaving the dryer is at 120 to 130 F., depending upon the type of copperas being dried. The temperatures in various parts of the dryer must remain constant. The temperature ofj the air leaving the dryer is controlled by means of an automatic gas controller with a droop corrector to offset changes in fuelv gas composition or changes in the quantity of gas required. The point oi control is the duct leading from the charge breeching to the cyclone. At this point, the temperature is maintained automatically at 120 to 130 F., within one degree.

The quantity of air admitted to the dryer must be constant. An automatic draft control device is employed to ensure accuracy in the feeding of the air. This device also corrects for changes in draft due to wind, etc. 'Ihe quantity of air supplied aiects the temperature at the end of the dryer where the material is discharged. This temperature is maintained at 200 to 250 F., as measured by an air thermometer located in the stream of dried copperas leaving the dryer. When the copperas vis heated under the conditions mentioned, G of its moisture is driven .o Without encountering the diiiiculties mentioned. 'I'he draft' required is usually 0.2 to 0.5 inch of Water in the air exit ue.

The quantity of air supplied also affects the Y rate of discharge offthe dried material. An excessof air causes/an excess of dust which blows out of the charge end, thus reducing the amount of material available at the discharge end. Also, the quantity of air controls the dewpoint at the air exit flue. If a suitable quantity of air is used, the dewpoint is low, and the flues remain clear. If too little air is used, the dewpoint is high, and moisture will condense out of it and cause accumulations of dust in the flue. Since a high dewpoint is desirable in the dryer proper, and undesirable in 'the ue, the dewpoint `is dropped in the flue by adding warm air at the point where the gases leave the dryer and enter the ue. Y

In the calciner, the material ows continuously from the feeding to the discharge end, but a substantial body of 'the material is retained in the calciner by the provision at the discharge end of a dam consisting of a circular plate with anopening at the center thereof. It is necessary to maintain a bed of material in order that overheating and consequent decomposition of manganese sulphate may be avoided. The material is heated by a flame and hot gases traveling concurrently with the material; vIn the rotating furnace, the material is constantly agitated so that fresh material comes into contact with the flame and hot gases only momentarily,

4 alegres troller which actuates a motor driven gas valve A which is in turn controlled by a thermocouple located inside the brick lining of the calciner.

The hot iron omde is discharged continuously,

and in quantity corresponding to that of the material entering at the feed end of the dryer,

into a Wash tank containing water which dissolves any soluble compound such as manganese sulphate. The iron oxide product may be recovered from the water in any suitable manner.

Owing to the eiect of control of the drying and calcining operations, the product will be found to be quite free from insoluble manganese compounds, that is, manganese will not exceed .05%. The gases from the calciner, consisting of sulphur dioxide and sulphur trioxide which re` sult from decomposition of the sulphate, pass through a cyclone in which any dust is separated, and thence to a stack from which the gases are discharged to the atmosphere.

Referring to the drawing, I have illustrated a suitable apparatus in which the method may be conducted, although numerous modifications may be employed in effecting the operation and control of the method.

The dryer 5 is a rotating steel cylinder adapted to be driven in any suitable manner from a source of power (not shown). It may, for example, be 6 feet in diameter and 40 feet in length. 'I'he copperas is fed from'a hopper S by conveyor 'i at a uniform rate, and is delivered to the-dryer which may be provided with iiights 8 to increase the contact of the copperas with the hot gases. A suitable fuel such as gas is supplied from a pipe 9 and branch i0 controlled by a valve Il. This is automatically actuated by a pneumatic controller l2 and droop corrector I3 which is connected to a bulb ill at the feed end of the dryer. The gas is burned in a combustion chamber i5 and passed through a chamber I6 into which additional air is supplied under control of dampers Il. The flame and hot gases pass into the dryer and travel' countercurrent to the copperas as it advances throughk the dryer. As hereinbefore indicated, the amounts of gas and air are carefully regulated to maintain the desired temperature gradient in the dryer. The temperature at the discharge end is controlled by the quantity of air drawn through the dryer by suction induced by a fan I8 which is oonnected by a flue I9 to the dryer and by a flue 20 to a cyclone 2l where dust is removed from the gases. A ue 22 permits introduction of warm air under control of a damper 23 which is actuated by a motor 24 controlled by a draft regulator 25, draft adjusting motor 26, droop corrector 21, and potentiometer 28, which is connected to a thermocouple 29. A hand-operated damper 30 is disposed in the flue to which 2,184,789 i u te nie meiner sa -wmeh is" a brick-uned steelcylinder adapted to beY rotated through any suit- Aable means from a source ofpower (not shown).

This furnace may be somewhat smaller than the dryer, because of the reduced volume of the material treated.. A suitablefuel such as gas is fed from the pipe 9 to the burner 40, air being introduced atthe feed end of the ca lciner through an opening surrounding the burner. The amount of gas is regulated by a. valve 4I actuated by a motor 42, which is controlled by'a droop corrector 43 and potentiometer 44, the latter being connected to a thermocouple 45 so as to maintain the desired temperature in the calciner.

The air is drawn into the calciner by the draft of a stack 46' connected to a cyclone 41. which is in turn connected by a flue 48 to the discharge end of the calciner. A rotoclone 49 and dust hopper 50 are provided to separate dust from the gases and to return the dust through a pipe i to a tank 52 into which the product is discharged. The draft is regulated bya regulator 53 actuated by the motor 42 which in turn controls a motor damper 54 actuating .a damper 55 in' an air inlet l'lue 56. With the regulation as described, it is possible to maintain the desired temperature or gradientcontrol in the calciner and to limit the temperfresh particles into contact with the hot flame and gases and avoiding overheating of the material. 'The calcined material constantly overilows 'the dam in proportion to the feed, and the material isdelivered to the tank 6 containing water which quenches the hot material and dissolves soluble constituents such as manganese ampliate. A pipe I8 and pump Il permit withiron oxide product.'

3 drawal ofth'e slurry or wet material which may be subsequently treated in any suitable apparagtus such as a filter (not shown) 'to recover the The product thus obtained by a continuous lor uninterrupted operation of drying and calcining.

is a red iron oxide of desirable shade having a low manganese content. It is of neftextureand after washing, drying and grinding', is suitable for use as a pigment and for various other purposes. Owing-to the continuous .operation and the elimination'of handling of the material, the product -is less expensive than decomposition products of copperas prepared by batch methods.

Various changes may be made ln the structure employed and inthe regulating and controlling devices, without departing from the invention or sacricinglthe advantages thereof.

I claim:

'I'he method of producing a red oxide of iron' of fine texture and purity from commercial copperas which comprises maintaining'an uninterrupted flow of finely divided copperas from a source of supply and subjecting the finely divided copperas during transit to drying at regulated temperature suillciently low that at nostage of the drying operation is the material being treated melted in its water of crystallization and is continuously maintained in its finely divided state,

to remove from the copperas six of its seven molecules of water, then transferring lthe resulting nely divided product to a rotating calcining zone and subjecting it during passage through said zone to heating gases at a regulated temperature sumciently' high to produce-ferrie oxide, maintaining a bed of material being calcined during caloination in said zone, and rotating the calcning zone at such rate that the material is mixed with the bed and is only momentarily exposed to the heated gases so that overheating is avoided, whereby ferrie oxide of a'ilneness suitable for pigment purposes, without grinding, is obtained. Y 

